声电沉积C/C磷灰石生物活性涂层的超声作用机制

采用声电沉积工艺在炭/炭复合材料表面制备了磷灰石生物活性涂层,借助SEM,EDAX,XRD,FTIR等分析测试手段,考察了超声频率对涂层组成、结构和形貌的影响.结果表明低超声频率时(25 kHz)形成片状羟基磷灰石(Ca10(PO4)6(OH)2(HA));当超声频率升高时(45 kHz或60 kHz)形成棒状磷酸氢钙(CaHPO4·2H2O(DCPD)).随着超声频率的升高,涂层呈紧密堆积并沿(021)、(041)晶面择优生长,涂层厚度和n(Ca)/n(P)逐渐减小,电解液的pH值逐渐升高.超声波对电沉积的作用主要是降低了钙磷相反应能垒和增强了类旋转效应.     

碳／碳复合材料表面声电沉积磷灰石动力学研究

采用声电沉积技术，在碳／碳复合材料表面制备了生物活性磷酸钙涂层。扫描电镜、X射线衍射、红外反射以及X射线能谱分析表明所制涂层呈现网状结构，其由钙磷比为1．64、含碳酸根的羟基磷灰石组成。根据扫描电镜观察，描述了磷灰石的形成过程。羟基磷灰石的沉积过程可简化为两步——钙磷离子向碳／碳阴极表面运动和羟基磷灰石在碳／碳表面生长。基于此描述，导出了羟基磷灰石沉积动力学公式，并且发现，沉积过程受扩散控制，扩散活化能是30．3kJ／mol．     

钛合金表面声电沉积／碱热处理法制备HA涂层研究

为了使钛合金（Ti-6Al-4V）具有生物活性，可在其表面施加生物活性羟基磷灰石（HA）涂层。对比了声电沉积法和碱热处理法实验结果，采用扫描电镜（SEM）、X射线衍射仪（XRD）、电子能谱（EDS）、傅立叶红外透射光谱（FTIR）以及划痕测试等进行了分析。结果表明，直接采用声电沉积法在钛合金表面制备的羟基磷灰石涂层，经热处理后存在龟裂剥落现象；通过碱热处理法，对钛合金基体表面进行预处理，然后，借助声电沉积法，在钛金属表面沉积了透钙磷石涂层，经热碱液处理转变成的羟基磷灰石涂层，涂层完整，未出现剥落。经进一步高温烧结处理，所制涂层仍呈片状形貌，其由部分含钠的羟基磷灰石组成，而且HA涂层破坏的临界载荷未烧结前的4．365N提高至烧结后的8．175N。     

声电沉积钙磷生物涂层工艺中超声波的作用机理研究

采用声电沉积工艺,在碳/碳复合材料表面制备了生物活性透钙磷石涂层工艺,借助SEM,EDAX,精密天平等分析手段,根据该涂层的沉积动力学规律,探讨了声电沉积工艺中,超声波在钙磷涂层形成中的作用机理.结果表明,在10～18 mA/cm2的范围内,随电流密度增加,透钙磷石涂层内晶粒仍呈片状,但尺寸逐渐减小,沉积速率依次增加;在沉积初期内,透钙磷石涂层沉积过程受扩散过程控制;声电沉积工艺中,超声波引入可导致界面附近扩散层内pH降低以及磷酸钙涂层沉积所需临界电荷密度降低,电流密度与诱导期之间符合Sand关系式.     

炭/炭复合材料抗氧化抗热震铱涂层的研究进展

铱是航天领域1800 ℃以上炭/炭复合材料抗氧化抗热震涂层的首选材料。本文介绍了物理气相沉积、金属有机物化学气相沉积、熔盐电解沉积和双层辉光等离子沉积等4种主要制备铱涂层的方法,讨论了铱涂层与炭/炭复合材料基体之间过渡层的材料选择,总结了铱涂层的地面试车测试结果,分析了影响铱涂层寿命的因素,指出今后我国制备铱涂层的技术途径应采用熔盐电解沉积 (Electroformed Deposition, 简写为ED)、双层辉光等离子沉积 (Double-glow Plasma Deposition, 简写为DPD)方法。     

炭/炭复合材料表面氢刻蚀改善等离子体渗Cr层的抗氧化性能

用双层辉光等离子渗金属技术,在炭/炭复合材料表面制备Cr涂层,改善其抗高温氧化性能。渗Cr前先用微波等离子体对炭/炭复合材料表面进行氢刻蚀处理,提高Cr涂层与基体间的结合力。用扫描电子显微镜、能谱仪和X-射线衍射仪分别对刻蚀、渗Cr及氧化后炭/炭复合材料表面形貌、成分及组织结构进行分析。结果表明:经过900℃、1 h刻蚀后,炭/炭复合材料表面形成蜂窝状结构,经后续950℃、2 h渗Cr处理后,在刻蚀后的炭/炭复合材料表面形成厚约5μm的Cr/Cr_yC_x复合涂层,涂层表面致密均匀,无裂纹和剥落;900℃高温循环氧化2.4 h后的失重率为2.79%,抗高温氧化能力较基材得到明显改善。     

碳纤维表面生长纳米碳管及其增强的炭/炭复合材料

采用化学气相沉积工艺在碳纤维表面生长了纳米碳管,将此种碳纤维作为增强材料,以中间相沥青为基体炭前驱体采用浸渍炭化工艺制备了炭/炭复合材料.观察了所得复合材料断口的微观形貌,测试了抗弯强度及热物理性能.结果表明,碳纤维表面的纳米碳管可以有效地提高纤维与基体的粘结力,复合材料的抗弯性能提高了50%,而对复合材料的导热性能影响较小.     

CVI炭/炭复合材料微观结构和生长模型

采用自行设计的多元耦合物理场CVI炉增密炭/炭（C/C）复合材料,用炭毡作为纤维增强体,在坯体内部设计特殊的导电发热层,使坯体内部的温度场、气体反应的中间产物浓度场、电磁场等多元物理场实现耦合,实现坯体的快速增密。采用偏光显微镜研究沉积热解炭的组织结构;用X射线衍射仪研究C/C复合材料的石墨化度和微晶尺寸;用扫描电镜观察材料断口和热解炭沉积表面的形貌;并对CVI热解炭的生长方式进行研究。研究表明：获得SL、RL和带状等多种热解炭结构;不同的结构具有不同的形貌特征,其中SL的断口平整,RL的断口呈沟槽构造;并提出前者为小分子平滑生长模型、后者为大分子锥状生长模型。     

钛合金表面声电沉积/碱热处理法制备HA涂层研究

为了使钛合金(Ti-6Al-4V)具有生物活性,可在其表面施加生物活性羟基磷灰石(HA)涂层.对比了声电沉积法和碱热处理法实验结果,采用扫描电镜(SEM)、X射线衍射仪(XRD)、电子能谱(EDS)、傅立叶红外透射光谱(FTIR)以及划痕测试等进行了分析.结果表明,直接采用声电沉积法在钛合金表面制备的羟基磷灰石涂层,经热处理后存在龟裂剥落现象;通过碱热处理法,对钛合金基体表面进行预处理,然后,借助声电沉积法,在钛金属表面沉积了透钙磷石涂层,经热碱液处理转变成的羟基磷灰石涂层,涂层完整,未出现剥落.经进一步高温烧结处理,所制涂层仍呈片状形貌,其由部分含钠的羟基磷灰石组成,而且HA涂层破坏的临界载荷未烧结前的4.365 N提高至烧结后的8.175N.     

微弧氧化法制备氧化钛基多孔复合生物陶瓷涂层

采用新颖的微弧氧化法(Microarc oxidation,MAO)在钛合金表面制备氧化钛基含钙磷的多孔复合生物陶瓷涂层.用扫描电镜(SEM)、电子能谱(EDAX)和X射线衍射(XRD)表征涂层的微观形貌、元素与相组成.采用纳米压痕仪(Nano Indenter)测试涂层的力学性能,并通过在模拟体液(Simulated body fluid,SBF)中培养对陶瓷涂层的生物活性进行了初步研究.结果表明,微弧氧化时间、电解液配比与电参数是影响涂层结构与Ca/P比值的关键工艺参数.涂层主要由锐钛矿和金红石相TiO2及钙磷化合物组成.涂层内层为致密的氧化钛层,并与钛合金基底成微冶金结合.涂层外层主要为含钙磷的化合物层,且涂层表面呈多微孔结构,有利于骨组织的长入并改善骨与植入体的结合.涂层的硬度为5.9GPa,弹性模量为102.5GPa.优化工艺参数下(氧化时间5min,占空比8%)制备的涂层,在模拟体液中培养8周有明显的羟基磷灰石沉积.羟基磷灰石在微孔内或孔边缘位置首先形核并长大,并逐渐向周边扩展生成羟基磷灰石层,体现了多孔含钙磷生物陶瓷涂层良好的诱骨生长特性.     

Effect of Substrate Temperature on CaHPO4 Coating on HT-C/C Composites Prepared by Ultrasonic Induction Heating Method

采用超声感应加热法在H2O2水热处理C/C复合材料表面沉积了CaHPO4涂层,借助SEM、XRD、FTIR、EDS等手段,研究了衬底温度对涂层的微观结构的影响,并通过划痕测试评价涂层与C/C基体之间的结合强度,同时运用分析天平测量质量以研究涂层的沉积动力学。结果显示,所制得的CaHPO4涂层钙磷比为1.2左右,晶格中出现碳离子。涂层形貌无明显变化,但是伴随温度的升高,涂层致密度降低。涂层与基体之间的结合强度随温度升高而增强,但内聚强度随温度升高而减弱。CaHPO4涂层的感应加热沉积过程受表面化学反应控制,沉积活化能为46.7 kJ/mol。     

工艺因素对水热改性C/C复合材料抗氧化性能的影响

以一定配比的Al_2O_3粉和磷酸溶液组成的悬浮液作为水热处理前驱体,采用水热法对C/C复合材料基体进行了防氧化改性.采用X射线衍射(XRD)仪、扫描电子显微镜(SEM)和能量色散谱(EDS)仪分别对改性试样的物相组成、显微结构及化学元素组成进行表征.重点研究了水热反应时间、水热反应釜填充比等工艺因素对改性C/C复合材料的物相组成、微观形貌及抗氧化性能的影响.结果表明:水热改性方法是一种行之有效的提高C/C复合材料基体抗氧化性能的手段.经过水热改性处理,试样的抗氧化性能明显提高;延长水热反应时间和增大水热釜填充比都有利于基体抗氧化性能的提高;在水热釜填充比为70%、水热温度为200 ℃的条件下,改性处理72 h的C/C复合材料在700 ℃的静态空气中恒温氧化10 h后氧化失重仅为2.31%.     

Effect of Mo/Si Ratio on the Microstructure and Oxidation Resistance of Si-Mo Coating for C/C Composites

Oxidation protective Si-Mo coatings were prepared by pack cementation on the surface of C/SiC coated carbon/carbon composites. The influences of Mo/Si mass ratio in the pack powders on the microstructure and oxidation resistance of the coating were investigated. It showed that with the Mo/Si ratio increasing from 0.1 to 0.4, the MoSi2 proportion and the dimension of cracks in the coating increased, and the oxidation protective ability of the coated specimens firstly increased and then decreased. The coating...     

Anti-oxidation behavior of chemical vapor reaction SiC coatings on different carbon materials at high temperatures

To protect carbon materials from oxidation, SiC coatings were prepared on carbon/carbon(C/C) composites and graphite by chemical vapor reaction. SEM and XRD analyses show that the coatings obtained are composed of SiC grains and micro-crystals. The influence of different carbon substrates on oxidation behavior of coated samples was investigated, and then their oxidation mechanisms were studied. Oxidation test shows that the SiC coated graphite has a better oxidation resistance than SiC coated C/C composites at high temperatures (1 623 K and 1 823 K). In the oxidation process, the oxidation curves of SiC coated C/C composites are linear, while those of SiC coated graphite follow a quasi-parabolic manner. The oxidation mechanism of the former is controlled by chemical reaction while the latter is controlled by oxygen diffusion based on the experimental results. The variation of oxidation behavior and mechanism of SiC coatings on two kinds of carbon substrates are primarily contributed to their structure differences.     

Ablation-resistant Ir/Re coating on C/C composites at ultra-high temperatures

An iridium/rhenium(Ir/Re)double-layer coating was prepared on carbon/carbon(C/C)composites by chemical vapor deposition(CVD)and electrodeposition.The morphologies and bond strengths of the coatings on the C/C substrate were examined.The ablation resistance of the Ir/Re coating was studied at 1800℃in an oxyacetylene torch flame for 300 s.The results show that Re interlayer increases the bond strength between Ir coating and C/C substrate by over 100%.During entire hightemperature ablation process,Ir/Re coating keeps intact without any signs of ablation damage.Ir coating gets smoother and the grain size becomes larger after ablation,with the preferred orientation changing from h311i to h220i:Although some voids are observed along the grain boundaries of the as-ablated Ir coating,Ir/Re coating keeps intact on C/C composites.The study indicates that Ir/Re coating can provide good ablation resistance up to 1800℃for C/C composites,especially for the continuous ablation applications.     

C/C复合材料高温抗烧蚀涂层的研究进展

C/C复合材料在高温燃气高速冲刷环境中的严重氧化烧蚀限制了其在航空航天等领域的广泛应用,采用抗烧蚀涂层技术是目前提高该材料高温抗烧蚀性能的有效方法。综述了近年来国内外C/C复合材料高温抗烧蚀涂层在玻璃涂层、金属涂层、陶瓷涂层等体系方面的研究进展,总结并评价了C/C复合材料抗烧蚀涂层的抗烧蚀性能测试技术及其研究成果,提出了C/C复合材料高温抗烧蚀涂层在未来研究中潜在的重点发展方向。     

Identification of the wear mechanism on WC/C nanostructured coatings

A series of WC/C nanostructured films with carbon contents ranging from 30 to 70 at.% was deposited on M2 steel substrates by magnetron sputtering of WC and graphite targets in argon. Depending on the amorphous carbon (a-C) incorporated in the coatings, nanocrystalline coating (formed mainly by WC_{1 − x} and W₂C phases) or nanocomposite (WC_{1 − x}/a-C) were obtained with tunable mechanical and tribological properties. Ultrahardness values of 36–40 GPa were measured for the nanocrystalline samples whilst values between 16 and 23 GPa were obtained in the nanocomposite ones depending on the a-C content. The tribological properties were studied using a pin-on-disk tester versus steel (100Cr6) balls and 5 N of applied load in dry sliding conditions and the failure modes by scratch adhesion tests. Three different zones were identified according to the observed tribological behavior: I (μ > 0.8; adhesive wear), II (μ: 0.3–0.6; abrasive wear) and III (μ ~ 0.2; self-lubricated). The wear tracks and the ball scars were observed by scanning electron microscopy (SEM) and Raman spectroscopy in order to elucidate the tribochemical reactions appearing at the contact and to determine the wear mechanism present in each type. A correlation among structure, crystalline phases, a-C content and tribomechanical properties could be established for the series of WC/C coatings and extended to understand the trends observed in the literature for similar coatings.     

多孔体制备工艺对C/C-SiC复合材料弯曲性能的影响

以针刺整体炭毡为坯体,采用CVD和树脂浸渍／炭化混合法增密制备了4种C／C多孔体,然后熔硅浸渗C／C多孔体制备了C／C-SiC复合材料;研究了不同炭涂层、高温热处理对C／C-SiC复合材料弯曲强度和断裂方式的影响。结果表明：热解炭涂层可减少制备过程中炭纤维的损伤,具有适中的界面结合强度,使复合材料的弯曲强度达到161．5MPa,表现出良好的“假塑性”;适当选择高温热处理工艺可制备弯曲性能较高,具有一定“假塑性”的C／C-SiC复合材料。     

The effect of plasma spraying power on the structure and mechanical properties of hydroxyapatite deposited onto carbon/carbon composites

This paper deals with the effect of plasma spraying power on hydroxyapatite (HA) coatings on carbon/carbon composites (C/C composites). The microstructure and phase composition of the as-sprayed coatings have been examined by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The shear strength of the HA coatings–C/C substrates was detected on a RGD-5 tensile testing machine. Results indicate that the melting extent and the shear strength of the coatings were evidently improved with the increasing of spraying power. Moreover, the amount of decomposed phases is increased and the content of crystalline HA of coatings was slightly changed. Observation of fracture surfaces shows that carbon fiber bundles can bond well with HA coatings using 40 kW spraying power.     

表面硅化对C/C复合材料组织结构的影响

采用表面固相渗硅工艺在C/C复合材料表面制备SiC涂层 ,研究了制备工艺对涂层和C/C复合材料组织结构的影响。结果表明 :硅化反应时间对C/C复合材料的SiC涂层厚度影响不大 ;C/C复合材料组织中热解碳基体与碳纤维相比 ,更易与Si反应生成SiC ,说明碳纤维的稳定性高于热解碳 ,Si通过界面和材料缺陷扩散深入基体内部。